scholarly journals Einkristallzüchtung und Röntgenstrukturanalyse polymerer 1:1-Komplexe von CuBr2 und CuCl2 mit Pyrazin aus Gelen / Crystal Growth in Gels and X-Ray Characterization of Polymeric 1:1-Complexes of CuBr2 and CuCl2 with Pyrazine

1989 ◽  
Vol 44 (5) ◽  
pp. 553-556 ◽  
Author(s):  
Th. Fetzer ◽  
A. Lentz ◽  
T. Debaerdemaeker

Single crystals of Cu(pz)Br2 and Cu(pz)Cl2 were grown by using gel methods with tetramethoxysilane as the gel-forming reagent. Thermal decomposition is interpreted. Crystal data for the bromo complex: monoclinic, space group C2/m with a = 1239.2(3) pm, b = 685.9(2) pm, c = 390.7(3) pm, β = 96,23(5)°. Crystal data for the chloro-complex: monoclinic, space group C2/m with a = 1197.1(3) pm, b = 684.9(3) pm, c = 370.1(3) pm, β = 95.96(5)°. Crystal structure analyses reveal that CuHal2 molecules are bonded by pyrazine to form linear chains. These chains are cross-linked by bridging halogen atoms.

1990 ◽  
Vol 45 (2) ◽  
pp. 199-202 ◽  
Author(s):  
Th. Fetzer ◽  
A. Lentz ◽  
T. Debaerdemaeker ◽  
O. Abou-El-Wafa

Single crystals of Cu(pdz)Cl2 were grown by using gel methods with tetramethoxysilane as the gel-forming reagent. Thermal decomposition is interpreted. Crystal data for the complex : monoclinic, space group C2/c with a = 938.3(3) pm, b = 1242.9(3) pm, c = 675.7(4) pm, β = 128.48(5)°. A crystal structure analysis reveals CuCl2 molecules connected by pyridazine in the form of zigzag-chains. Between these chains there are only Van-der-Waals-Interactions.


1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2


2019 ◽  
Vol 74 (4) ◽  
pp. 381-387
Author(s):  
Michael Zoller ◽  
Jörn Bruns ◽  
Gunter Heymann ◽  
Klaus Wurst ◽  
Hubert Huppertz

AbstractA potassium tetranitratopalladate(II) with the composition K2[Pd(NO3)4] · 2HNO3 was synthesized by a simple solvothermal process in a glass ampoule. The new compound crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 1017.15(4), b = 892.94(3), c = 880.55(3) Å, and β = 98.13(1)° (Z = 2). The crystal structure of K2[Pd(NO3)4] · 2HNO3 reveals isolated complex [Pd(NO3)4]2− anions, which are surrounded by eight potassium cations and four HNO3 molecules. The complex anions and the cations are associated in layers which are separated by HNO3 molecules. K2[Pd(NO3)4] · 2HNO3 can thus be regarded as a HNO3 intercalation variant of β-K2[Pd(NO3)4]. The characterization is based on single-crystal X-ray and powder X-ray diffraction.


1989 ◽  
Vol 44 (8) ◽  
pp. 903-910 ◽  
Author(s):  
Astrid Görge ◽  
Ute Patt-Siebel ◽  
Ulrich Müller ◽  
Kurt Dehnicke

[WCl4(NCl)]2 reacts in acetonitrile with the trimethylsilyl compounds Me3SiSR (R = Me, Ph), and Me3SiESiMe3 (E = S, Se), with substitution of the chlorine atom of the N-chloronitreno group W=N–Cl and formation of CH3CN–WCl4(NSR) and CH3CN–WCl4(NEN)WCl4–NCCH3, respectively. Excess Me3SiBr reacts with CH3CN–WCl4(NSMe) to afford CH3CN–WBr4(NSMe). [CH3CN–WNCl3]4 was obtained from CH3CN–WCl4(NCl) and N(SiMe3)3. The products were characterized by their IR spectra. Two X-ray crystal structure determinations were also carried out. CH3CN—WCl4(NSMe) forms twinned crystals, and only non-overlapping reflexions of one of the twin individuals were used for the structure determination (846 unique values, R = 0.055). Crystal data: a = 592.4(2), b = 758.8(2), c = 1203.7(8) pm, β = 95.06(4)°, monoclinic, space group P21/m, Z = 2. The compound is a monomer in which the acetonitrile ligand is situated in the trans position to the W≡N–S̱̅–Me group. The bond lengths (W≡N 174(2), N–S 161(2) pm) and bond angles (WNS 176(1), NSC 102.1(9)°) are in agreement with the proposed formula. Crystal data for [CH3CN–WNCl3]4: a = 1009.5(2), b = 1274.5(2), c = 1287.9(2) pm, β = 108.17(1)°, monoclinic, space group P21/c, Z = 2 (2113 unique reflexions, R = 0.057). The compound forms tetrameric units, in which the W atoms form a square and are linked with one another via N atoms at alternating distances (W=N 171(2), W–N 207(2), W–NCMe 238(2) pm).


1987 ◽  
Vol 42 (7) ◽  
pp. 828-834 ◽  
Author(s):  
W. Frank ◽  
B. Dincher

Abstract The crystalline compounds [(CH3C6H5)2Hg,][AlCl4]2 (1), [(1,2-(CH3)2C6H4)2Hg2][AlCl4]2(2), [(1,3,5-(CH3)3C6H3)2Hg2][AlCl4]2 (3), [1,2,4,5-(CH3)4C6H2Hg2][AlCl4]2 (4) and [((CH3)6C6)2Hg2][AlCl4]2-CH3C6H5 (5) have been prepared from mercury(I)chloride, aluminium trichloride and the corresponding arenes and characterized by elem ental analysis. The crystal structure of 5 has been determ ined from single crystal X-ray diffraction data and refined to R - 0.093 for 3269 unique reflections. Crystal data: monoclinic, space group P21/c, a = 2116(1), b = 1095.1(7), c = 1880(1) pm, β - 104,9(1)°, Z = 4. Each atom of a central Hg2 unit (Hg -Hg distance 251.5 pm) is asymmetrically complexed by hexamethylbenzene, the Hg - Carene distances being in the range from 241 to 340 pm. Two distorted AlCl4 tetrahedra complete a “molecular” [arene2Hg2][AlCl4]2 unit. The shortest Hg-Cl distances are 310 and 312 pm, respectively.


1992 ◽  
Vol 70 (3) ◽  
pp. 703-709 ◽  
Author(s):  
Neil Burford ◽  
Trenton M. Parks ◽  
Bruce W. Royan ◽  
John F. Richardson ◽  
Peter S. White

Tetrachloroaluminate salts of the benzothiazarsolium and toluodithiarsolium heteronaphthalenic cations have been prepared from the corresponding chloroarsoles by a routine halide ion abstraction procedure. Characterization data are presented, including the X-ray crystal structure of the thiaza derivative. (Crystal data for C6H5AlAsCl4NS: monoclinic, space group P21/c, a = 6.4259(5) Å, b = 23.654(3) Å, c = 8.5859(7) Å, β = 98.203(6)°, V = 1291.7(2) Å3, Z = 4, R = 0.054.) A planar bicyclic cationic unit is observed, typical of other heteronaphthalenic systems. The crystal structure of 2-chlorobenzo-1,3,2-thiazarsole has been obtained for direct comparison, and also has a close to planar heterobicyclic moiety. (Crystal data for C6H5AsClNS: monoclinic, space group P21/c, a = 8.370(3) Å, b = 10.829(3) Å, c = 8.756(2) Å, β = 95.99(2)°, V = 789.2(3) Å3, Z = 4, R = 0.025.) The planarity and short heterocyclic bond lengths observed in the two compounds imply a significant degree of pπ bonding, which is unique between sulfur and arsenic. In addition, the cation is a rare example of a structurally characterized cationic dicoordinate arsenic, or arsenium, system. Keywords: arsenic, arsolium, arsenium, pπ-bonding, sulfur, heteronaphthalenic.


2013 ◽  
Vol 2013 ◽  
pp. 1-4 ◽  
Author(s):  
Mohamed I. Attia ◽  
Hazem A. Ghabbour ◽  
Maha S. Almutairi ◽  
Soraya W. Ghoneim ◽  
Hatem A. Abdel-Aziz ◽  
...  

Synthesis and characterization of (1E)-1-(4-chlorophenyl)-N-hydroxy-3-(1H-imidazol-1-yl)propan-1-imine (4) are reported. X-ray crystal structure of the title oxime4confirmed its assigned (E)-configuration. The compound crystallizes in the monoclinic space groupP21/cwitha=13.4292(3) Å,b=8.8343(2) Å,c=11.1797(3) Å,α=90°,β=108.873(2)°,γ=90°,V=1255.03(5) Å3, andZ=4. The molecules are packed in crystal structure by weak intermolecularO–H⋯Nhydrogen bonding interactions. Compound4is a useful intermediate for the synthesis of new imidazole-containing antifungal agents.


1986 ◽  
Vol 41 (7) ◽  
pp. 831-833 ◽  
Author(s):  
Wolfgang Willing ◽  
Ruth Christophersen ◽  
Ulrich Müller ◽  
Kurt Dehnicke

AbstractVBr2(N3S2)(pyridine)2 is obtained in form of brown-black, moisture sensitive crystals by the reaction of the corresponding chloro complex with trim ethylbrom osilane. The com pound is characterized by its IR spectrum and an X-ray crystal structure determination (1322 observed reflexions, R = 0.077). Crystal data: monoclinic, space group Aba2, Z = 4, a = 1100.3, b = 1480.0, c = 983.3 pm. A molecular structure with a distorted octahedral coordination for the vanadium atoms was found: there are two short VN bonds o f 178 pm with two N atoms o f the planar N3S2 chelate, two long (228 pm) VN(pyridine) bonds trans to the former VN bonds and two bromo ligands.


2013 ◽  
Vol 848 ◽  
pp. 195-198
Author(s):  
Zhi Xiang Ji

The crystals of 4,4-diaminodiphenyl sulfoxide have been obtained by evaporation from ethanol solution. The crystal structure of the 4,4-diaminodiphenyl sulfoxide was determined by X-ray single crystal diffraction analysis. The crystal data for 4,4-diaminodiphenyl sulfoxide: monoclinic, space groupP2(1)/c,a= 49.068(10) Å,b= 11.439(2) Å,c= 13.103(3) Å,V= 7347(3) Å3,Z= 24,Mr= 248.30,De= 1.347 g/cm3,T= 298(2) K,F(000) = 3120,R= 0.0786 andwR =0.2653. The compound forms three-dimensional network structure through hydrogen bonds and π-π interaction.


1989 ◽  
Vol 44 (5) ◽  
pp. 560-564 ◽  
Author(s):  
Gerhard Baum ◽  
Arnd Greiling ◽  
Werner Massa ◽  
Benjamin C. Hui ◽  
Jörg Lorberth

Reaction of Et3As with AsCl3 in n-pentane yields dimeric [Et3AsxAsCl3]2 in quantitative yield; sublimation in vacuo affords white crystals.X-Ray diffraction data were collected at 133 K (3149 independent observed reflections; R = 0.029. Rw = 0.026). Crystal data: monoclinic space group P21/c, a = 761.9(8). b = 1118.8(4). c = 1406.0(14) pm; β = 100.90(4)°. Ζ = 2 dimers.The dimer contains a planar As2Cl6-unit with terminal and bridging As-Cl bonds; each arsenic atom is bonded to a Et3As molecule via an arsenic-arsenic bond. The dimer thus has pseudo four- and six-coordinate arsenic atoms.


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